Sodium Hydroxide → 4-Amino-1-naphthaldehyde

HRID 1166788

反応式

HRID 1166788 の反応式
[S].[N+:2]([C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([CH3:15])=[CH:7][CH:6]=1)([O-])=O.[OH-:16].[Na+]>C(O)C.C(OCC)(=O)C>[NH2:2][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([CH:15]=[O:16])=[CH:7][CH:6]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 701554-Methyl-1-nitronaphthaleneHCID 5362487Sulfur

生成物 1

HCID 229991604-Amino-1-naphthaldehyde

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a stirring boiling solution of sulfur (3.7 g) in 12% aqueous NaOH (50 mL) was added a solution of 4-nitro-1-methylnaphthalene (8 g) in ethanol (50 mL). After refluxing the solution for one hour, the reaction was diluted with 500 mL of ethyl acetate and washed with water and brine, dried over MgSO4, and concentrated. The product was purified via silica gel column chromatography using ethyl acetate:hexane (5:95 to 10:90). The product (2.54 g, 34%) was stored at −78° C.

後処理

  1. temperatureAfter refluxing the solution for one hour
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe product was purified via silica gel column chromatography
  6. customwas stored at −78° C.

出典と根拠

ORDレコード
ord-8d668a3fd8f045c186ceef8d2ef27b55
出典データセット
uspto-grants-2003_09
特許番号
US06613942B1

関連ノート

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